+++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + SHELXL-97 - CRYSTAL STRUCTURE REFINEMENT - WinGX VERSION + + Copyright(C) George M. Sheldrick 1993-7 Release 97-2 + + 2008src0076 started at 10:21:25 on 29-Feb-2008 + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ TITL 2008src0076 in P2(1)2(1)2(1) CELL 0.71073 9.7751 12.8596 16.8243 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0004 0.0004 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H B N O F UNIT 88 100 4 8 4 16 V = 2114.88 F(000) = 880.0 Mu = 0.10 mm-1 Cell Wt = 1681.00 Rho = 1.320 MERG 4 OMIT -3.00 55.00 OMIT 1 0 3 SHEL 7 0.77 dfix 31 0.015 B1 F1 B1 F2 B1 F3 B1 F4 B11 F11 B11 F12 B11 F13 B11 F14 dang 31.6332 0.015 f1 f2 f1 f3 f1 f4 f2 f4 f3 f4 dang 31.6332 0.015 f11 f12 f11 f13 f11 f14 f12 f14 f13 f14 DFIX 31 0.015 B21 F21 B21 F22 B21 F24 B21 F23 DANG 31.6332 0.015 F21 F22 F21 F24 F21 F23 F22 F23 F24 F23 F22 F24 EADP B1 B11 B21 EADP F1 F11 F21 DELU 0.02 B1 > F24 SIMU 0.02 B1 > F24 sump 1 0.0000001 1 2 1 4 1 5 FMAP 2 PLAN 5 SIZE 0.17 0.24 0.28 ACTA BOND $H WGHT 0.05110 0.52860 L.S. 35 TEMP -153.00 FVAR 0.92867 0.66318 1.37490 0.15893 0.17787 MOLE 1 C1 1 0.329786 0.818853 0.956707 11.00000 0.02769 0.01919 = 0.02219 -0.00133 0.00042 -0.00197 C2 1 0.477920 0.820877 0.930619 11.00000 0.02928 0.02186 = 0.01625 0.00278 0.00236 0.00537 AFIX 13 H2 2 0.518106 0.749497 0.933939 11.00000 -1.20000 AFIX 0 C3 1 0.322185 0.884166 0.824704 11.00000 0.01872 0.02170 = 0.02250 0.00074 0.00071 0.00199 C4 1 0.271634 0.817133 0.755856 11.00000 0.02623 0.03078 = 0.02728 -0.00588 -0.00165 -0.00028 AFIX 137 H4A 2 0.296095 0.744341 0.765618 11.00000 -1.50000 H4B 2 0.314339 0.840647 0.706315 11.00000 -1.50000 H4C 2 0.172007 0.823366 0.751423 11.00000 -1.50000 AFIX 0 C5 1 0.313400 0.999617 0.804924 11.00000 0.02563 0.02274 = 0.02596 0.00262 -0.00216 0.00372 AFIX 137 H5A 2 0.220240 1.016553 0.787730 11.00000 -1.50000 H5B 2 0.377909 1.015976 0.762124 11.00000 -1.50000 H5C 2 0.336402 1.040566 0.852197 11.00000 -1.50000 AFIX 0 C6 1 0.105850 0.879082 0.909533 11.00000 0.02073 0.03852 = 0.03782 0.00150 0.00515 0.00045 AFIX 137 H6A 2 0.081157 0.867658 0.965308 11.00000 -1.50000 H6B 2 0.052217 0.832385 0.875651 11.00000 -1.50000 H6C 2 0.086499 0.951406 0.895018 11.00000 -1.50000 AFIX 0 C7 1 0.561891 0.897228 0.981871 11.00000 0.02186 0.03479 = 0.02369 -0.00222 -0.00157 0.00543 AFIX 23 H7A 2 0.561712 0.872228 1.037525 11.00000 -1.20000 H7B 2 0.657824 0.896767 0.963011 11.00000 -1.20000 AFIX 0 C8 1 0.509584 1.007699 0.980349 11.00000 0.02494 0.02827 = 0.02013 -0.00232 -0.00349 -0.00244 C9 1 0.576910 1.082945 0.935881 11.00000 0.02733 0.04235 = 0.03068 -0.00092 0.00088 -0.01305 AFIX 43 H9 2 0.659559 1.065628 0.909287 11.00000 -1.20000 AFIX 0 C10 1 0.524916 1.183350 0.929767 11.00000 0.05409 0.03324 = 0.03230 0.00392 -0.00810 -0.02336 AFIX 43 H10 2 0.572553 1.233987 0.899364 11.00000 -1.20000 AFIX 0 C11 1 0.404407 1.209882 0.967644 11.00000 0.06210 0.02317 = 0.02980 -0.00355 -0.01311 -0.00288 AFIX 43 H11 2 0.367772 1.277949 0.962298 11.00000 -1.20000 AFIX 0 C12 1 0.337672 1.136302 1.013425 11.00000 0.04210 0.02980 = 0.02932 -0.00611 -0.00048 0.00463 AFIX 43 H12 2 0.255549 1.154316 1.040298 11.00000 -1.20000 AFIX 0 C13 1 0.389980 1.036177 1.020366 11.00000 0.03057 0.02463 = 0.02428 0.00017 0.00343 -0.00092 AFIX 43 H13 2 0.343994 0.986629 1.052619 11.00000 -1.20000 AFIX 0 C14 1 0.561049 0.843687 0.793045 11.00000 0.02619 0.01956 = 0.01919 0.00071 0.00087 0.00047 AFIX 43 H14 2 0.542720 0.871374 0.741789 11.00000 -1.20000 AFIX 0 C15 1 0.690049 0.795173 0.804725 11.00000 0.02153 0.02378 = 0.02126 0.00056 -0.00066 0.00240 AFIX 43 H15 2 0.719964 0.774437 0.856058 11.00000 -1.20000 AFIX 0 C16 1 0.768500 0.779794 0.739412 11.00000 0.02101 0.02171 = 0.02405 0.00049 -0.00229 -0.00107 AFIX 43 H16 2 0.741741 0.815437 0.692461 11.00000 -1.20000 AFIX 0 C17 1 0.889275 0.714465 0.733729 11.00000 0.01864 0.02058 = 0.02463 -0.00102 0.00154 -0.00265 C18 1 0.939757 0.657444 0.798273 11.00000 0.02248 0.02748 = 0.02240 -0.00007 0.00091 0.00036 AFIX 43 H18 2 0.900318 0.666217 0.849443 11.00000 -1.20000 AFIX 0 C19 1 1.047251 0.588093 0.787842 11.00000 0.02498 0.02902 = 0.02695 0.00236 -0.00281 0.00390 AFIX 43 H19 2 1.080927 0.549327 0.831746 11.00000 -1.20000 AFIX 0 C20 1 1.105638 0.575471 0.712840 11.00000 0.02161 0.02611 = 0.03833 -0.00275 0.00275 0.00308 AFIX 43 H20 2 1.178800 0.527755 0.705678 11.00000 -1.20000 AFIX 0 C21 1 1.057269 0.632357 0.648608 11.00000 0.02522 0.03065 = 0.02878 -0.00274 0.00525 -0.00037 AFIX 43 H21 2 1.097394 0.623474 0.597629 11.00000 -1.20000 AFIX 0 C22 1 0.950578 0.702082 0.658676 11.00000 0.02375 0.02891 = 0.02257 0.00092 0.00164 -0.00081 AFIX 43 H22 2 0.918721 0.741660 0.614737 11.00000 -1.20000 AFIX 0 N1 4 0.251853 0.857855 0.898503 11.00000 0.02143 0.02207 = 0.02461 0.00070 0.00339 0.00151 N2 4 0.465975 0.853410 0.846531 11.00000 0.02124 0.01926 = 0.01939 0.00043 0.00104 0.00443 O1 5 0.291019 0.790381 1.022576 11.00000 0.03722 0.02812 = 0.02323 0.00330 0.00649 -0.00447 MOLE 2 PART 1 B1 3 0.581410 1.015005 0.605247 21.00000 0.03815 0.03056 = 0.03386 0.01144 -0.01014 -0.00605 F1 6 0.472416 0.946751 0.617890 21.00000 0.05154 0.04981 = 0.04959 -0.00089 0.00409 -0.01574 F2 6 0.604330 1.028426 0.525970 21.00000 0.03763 0.12138 = 0.04394 0.03450 -0.00310 -0.00376 F3 6 0.694655 0.969496 0.640956 21.00000 0.05737 0.04808 = 0.09387 0.03389 -0.04090 -0.00671 F4 6 0.556815 1.106617 0.642912 21.00000 0.12590 0.02794 = 0.11040 -0.00808 -0.00148 0.00224 PART 2 same b1 > f4 B11 3 0.597707 1.011873 0.615259 41.00000 0.03815 0.03056 = 0.03386 0.01144 -0.01014 -0.00605 F11 6 0.491063 0.941924 0.615502 41.00000 0.05154 0.04981 = 0.04959 -0.00089 0.00409 -0.01574 F12 6 0.589790 1.078481 0.552840 41.00000 0.09411 0.05468 = 0.07341 0.04494 0.00803 0.00611 F13 6 0.718283 0.958323 0.603730 41.00000 0.03949 0.04343 = 0.05864 0.00100 0.01213 0.00496 F14 6 0.601061 1.065276 0.685415 41.00000 0.05195 0.05484 = 0.07906 -0.04017 0.00912 -0.01458 PART 3 same b1 > f4 B21 3 0.562364 1.013782 0.609682 51.00000 0.03815 0.03056 = 0.03386 0.01144 -0.01014 -0.00605 F21 6 0.488541 0.921942 0.615433 51.00000 0.05154 0.04981 = 0.04959 -0.00089 0.00409 -0.01574 F22 6 0.626674 1.017963 0.537845 51.00000 0.05011 0.12097 = 0.06462 0.02549 0.02933 -0.01654 F23 6 0.657437 1.015494 0.670128 51.00000 0.07341 0.05547 = 0.09318 0.01888 -0.04284 -0.00532 F24 6 0.471041 1.093413 0.618872 51.00000 0.11193 0.02995 = 0.05377 0.02050 0.01349 0.04086 HKLF 4 Covalent radii and connectivity table for 2008src0076 in P2(1)2(1)2(1) C 0.770 H 0.320 B 0.820 N 0.700 O 0.660 F 0.640 C1 - O1 N1 C2 C2 - N2 C1 C7 C3 - N1 N2 C5 C4 C4 - C3 C5 - C3 C6 - N1 C7 - C8 C2 C8 - C9 C13 C7 C9 - C8 C10 C10 - C11 C9 C11 - C10 C12 C12 - C11 C13 C13 - C12 C8 C14 - N2 C15 C15 - C16 C14 C16 - C15 C17 C17 - C18 C22 C16 C18 - C19 C17 C19 - C18 C20 C20 - C21 C19 C21 - C22 C20 C22 - C21 C17 N1 - C1 C3 C6 N2 - C14 C2 C3 O1 - C1 B1_a - F4_a F2_a F3_a F1_a F1_a - B1_a F2_a - B1_a F3_a - B1_a F4_a - B1_a B11_b - F12_b F14_b F11_b F13_b F11_b - B11_b F12_b - B11_b F13_b - B11_b F14_b - B11_b B21_c - F22_c F24_c F23_c F21_c F21_c - B21_c F22_c - B21_c F23_c - B21_c F24_c - B21_c 18843 Reflections read, of which 65 rejected -11 =< h =< 12, -16 =< k =< 16, -21 =< l =< 21, Max. 2-theta = 54.96 0 Systematic absence violations 0 Inconsistent equivalents 2740 Unique reflections, of which 0 suppressed R(int) = 0.0552 R(sigma) = 0.0381 Friedel opposites merged Maximum memory for data reduction = 3705 / 26615 Default effective X-H distances for T = -153.0 C AFIX m = 1 2 3 4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16 d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95 Note that these distances are chosen to give the best fit to the X-ray data and so avoid the introduction of systematic error. The true internuclear distances are longer and do not vary with temperature ! The apparent variation with temperature is caused by libration. Least-squares cycle 1 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1030 before cycle 1 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 1 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.010 0.030 0.000 0.000 GooF = S = 1.051; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92899 0.00193 0.168 OSF 2 0.66346 0.00374 0.075 FVAR 2 3 1.37478 0.00292 -0.040 FVAR 3 4 0.15818 0.00732 -0.102 FVAR 4 5 0.17834 0.00753 0.063 FVAR 5 Mean shift/esd = 0.048 Maximum = 0.351 for U12 F24_c Max. shift = 0.002 A for F23_c Max. dU = 0.001 for F24_c Least-squares cycle 2 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 2 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 2 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 0.084 OSF 2 0.66383 0.00375 0.098 FVAR 2 3 1.37476 0.00292 -0.007 FVAR 3 4 0.15769 0.00731 -0.068 FVAR 4 5 0.17847 0.00752 0.017 FVAR 5 Mean shift/esd = 0.017 Maximum = -0.128 for U11 F14_b Max. shift = 0.001 A for F13_b Max. dU = 0.000 for F14_b Least-squares cycle 3 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1028 before cycle 3 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 3 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 0.007 OSF 2 0.66416 0.00374 0.089 FVAR 2 3 1.37476 0.00292 -0.002 FVAR 3 4 0.15748 0.00729 -0.028 FVAR 4 5 0.17841 0.00750 -0.008 FVAR 5 Mean shift/esd = 0.004 Maximum = 0.089 for FVAR 2 Max. shift = 0.001 A for F14_b Max. dU = 0.000 for F14_b Least-squares cycle 4 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 4 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 4 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 0.001 OSF 2 0.66447 0.00374 0.084 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15734 0.00728 -0.020 FVAR 4 5 0.17820 0.00749 -0.028 FVAR 5 Mean shift/esd = 0.003 Maximum = 0.084 for FVAR 2 Max. shift = 0.001 A for F21_c Max. dU = 0.000 for F24_c Least-squares cycle 5 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 5 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 5 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 0.000 OSF 2 0.66476 0.00374 0.078 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15722 0.00727 -0.016 FVAR 4 5 0.17800 0.00749 -0.027 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.078 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 6 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 6 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 6 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 -0.001 OSF 2 0.66504 0.00374 0.074 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15714 0.00727 -0.011 FVAR 4 5 0.17780 0.00748 -0.026 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.074 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 7 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 7 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 7 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 -0.001 OSF 2 0.66530 0.00374 0.070 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15707 0.00726 -0.010 FVAR 4 5 0.17761 0.00747 -0.025 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.070 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 8 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 8 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 8 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 0.000 OSF 2 0.66555 0.00374 0.066 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15701 0.00726 -0.008 FVAR 4 5 0.17742 0.00747 -0.025 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.066 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 9 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 9 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 9 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92917 0.00193 -0.001 OSF 2 0.66578 0.00374 0.062 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15696 0.00726 -0.007 FVAR 4 5 0.17724 0.00747 -0.024 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.062 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 10 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 10 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 10 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 -0.001 OSF 2 0.66600 0.00374 0.059 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15692 0.00725 -0.006 FVAR 4 5 0.17706 0.00746 -0.024 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.059 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 11 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 11 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 11 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 -0.001 OSF 2 0.66621 0.00374 0.056 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15688 0.00725 -0.006 FVAR 4 5 0.17690 0.00746 -0.022 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.056 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 12 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 12 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 12 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 -0.001 OSF 2 0.66640 0.00374 0.053 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15685 0.00724 -0.004 FVAR 4 5 0.17673 0.00745 -0.022 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.053 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 13 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 13 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 13 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.050; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 -0.001 OSF 2 0.66659 0.00374 0.050 FVAR 2 3 1.37476 0.00292 0.000 FVAR 3 4 0.15681 0.00724 -0.005 FVAR 4 5 0.17658 0.00745 -0.020 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.050 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 14 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 14 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 14 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 -0.001 OSF 2 0.66677 0.00374 0.047 FVAR 2 3 1.37475 0.00292 0.000 FVAR 3 4 0.15678 0.00724 -0.004 FVAR 4 5 0.17643 0.00744 -0.020 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.047 for FVAR 2 Max. shift = 0.001 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 15 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 15 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 15 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 0.000 OSF 2 0.66694 0.00374 0.045 FVAR 2 3 1.37475 0.00292 0.000 FVAR 3 4 0.15676 0.00724 -0.004 FVAR 4 5 0.17629 0.00744 -0.019 FVAR 5 Mean shift/esd = 0.002 Maximum = 0.045 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 16 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 16 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 16 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92916 0.00193 -0.001 OSF 2 0.66709 0.00374 0.042 FVAR 2 3 1.37475 0.00292 0.000 FVAR 3 4 0.15673 0.00723 -0.003 FVAR 4 5 0.17616 0.00744 -0.018 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.042 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 17 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 17 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 17 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66724 0.00374 0.040 FVAR 2 3 1.37475 0.00293 0.000 FVAR 3 4 0.15671 0.00723 -0.003 FVAR 4 5 0.17603 0.00744 -0.017 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.040 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 18 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 18 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 18 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66739 0.00374 0.038 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15669 0.00723 -0.003 FVAR 4 5 0.17591 0.00743 -0.017 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.038 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 19 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 19 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 19 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66752 0.00374 0.036 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15667 0.00723 -0.003 FVAR 4 5 0.17580 0.00743 -0.015 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.036 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 20 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 20 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 20 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66765 0.00374 0.035 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15665 0.00723 -0.003 FVAR 4 5 0.17568 0.00743 -0.015 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.035 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 21 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 21 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 21 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66778 0.00374 0.033 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15662 0.00722 -0.003 FVAR 4 5 0.17558 0.00742 -0.013 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.033 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 22 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 22 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 22 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66789 0.00374 0.031 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15661 0.00722 -0.002 FVAR 4 5 0.17548 0.00742 -0.014 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.031 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 23 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 23 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 23 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 0.000 OSF 2 0.66800 0.00374 0.029 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15660 0.00722 -0.002 FVAR 4 5 0.17539 0.00742 -0.013 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.029 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 24 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 24 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 24 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 0.000 OSF 2 0.66811 0.00374 0.028 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15658 0.00722 -0.002 FVAR 4 5 0.17530 0.00742 -0.012 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.028 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 25 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 25 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 25 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92915 0.00193 -0.001 OSF 2 0.66821 0.00374 0.027 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15656 0.00722 -0.002 FVAR 4 5 0.17521 0.00742 -0.012 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.027 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 26 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 26 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 26 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 -0.001 OSF 2 0.66830 0.00374 0.025 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15655 0.00721 -0.002 FVAR 4 5 0.17514 0.00741 -0.011 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.025 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 27 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 27 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 27 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 0.000 OSF 2 0.66839 0.00374 0.024 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15654 0.00721 -0.002 FVAR 4 5 0.17506 0.00741 -0.010 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.024 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 28 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1028 before cycle 28 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 28 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.009 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 0.000 OSF 2 0.66847 0.00374 0.022 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15652 0.00722 -0.002 FVAR 4 5 0.17499 0.00741 -0.010 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.022 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 29 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 29 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 29 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 0.000 OSF 2 0.66855 0.00374 0.021 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15651 0.00721 -0.002 FVAR 4 5 0.17492 0.00741 -0.009 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.021 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 30 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 30 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 30 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 0.000 OSF 2 0.66863 0.00374 0.020 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15650 0.00721 -0.001 FVAR 4 5 0.17485 0.00741 -0.009 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.020 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 31 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 31 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 31 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 -0.001 OSF 2 0.66870 0.00374 0.020 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15650 0.00721 -0.001 FVAR 4 5 0.17479 0.00741 -0.009 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.020 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 32 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 32 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 32 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 0.000 OSF 2 0.66877 0.00374 0.019 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15648 0.00721 -0.002 FVAR 4 5 0.17473 0.00740 -0.007 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.019 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 33 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 33 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 33 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 0.001 OSF 2 0.66884 0.00374 0.018 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15647 0.00721 -0.001 FVAR 4 5 0.17468 0.00740 -0.008 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.018 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 34 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 34 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 34 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 -0.001 OSF 2 0.66890 0.00374 0.016 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15646 0.00721 -0.001 FVAR 4 5 0.17462 0.00740 -0.007 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.016 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Least-squares cycle 35 Maximum vector length = 511 Memory required = 4676 / 436635 wR2 = 0.1029 before cycle 35 for 2740 data and 344 / 344 parameters Summary of restraints applied in cycle 35 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 N value esd shift/esd parameter 1 0.92914 0.00193 -0.001 OSF 2 0.66896 0.00374 0.016 FVAR 2 3 1.37476 0.00293 0.000 FVAR 3 4 0.15645 0.00721 -0.002 FVAR 4 5 0.17458 0.00740 -0.006 FVAR 5 Mean shift/esd = 0.001 Maximum = 0.016 for FVAR 2 Max. shift = 0.000 A for F22_c Max. dU = 0.000 for F24_c Largest correlation matrix elements 0.876 z F21_c / U23 F1_a -0.755 z F3_a / FVAR 5 -0.686 z F14_b / y F14_b -0.869 FVAR 5 / FVAR 4 0.750 z F23_c / z F22_c 0.685 U11 F22_c / x F2_a -0.815 y F11_b / y F1_a -0.746 U23 F1_a / z F1_a -0.684 U13 F3_a / U11 F3_a 0.796 x F13_b / x F11_b -0.733 z F21_c / z F1_a -0.678 y F22_c / z F21_c 0.791 U13 F1_a / z F1_a -0.732 y F22_c / y F2_a -0.675 x F4_a / FVAR 4 0.786 U11 F1_a / x F1_a 0.732 y F13_b / U23 F3_a -0.674 y F11_b / x F11_b 0.773 z F14_b / z F12_b 0.702 x F4_a / FVAR 5 0.672 x F13_b / x B11_b 0.766 z F3_a / FVAR 4 -0.689 x F13_b / U11 F3_a -0.667 U12 F1_a / x F1_a Idealized hydrogen atom generation before cycle 36 Name x y z AFIX d(X-H) shift Bonded to Conformation determined by H2 0.5181 0.7495 0.9339 13 1.000 0.000 C2 N2 C1 C7 H4A 0.2960 0.7443 0.7656 137 0.980 0.000 C4 C3 H4A H4B 0.3144 0.8406 0.7063 137 0.980 0.000 C4 C3 H4A H4C 0.1720 0.8234 0.7514 137 0.980 0.000 C4 C3 H4A H5A 0.2202 1.0165 0.7877 137 0.980 0.000 C5 C3 H5A H5B 0.3779 1.0160 0.7621 137 0.980 0.000 C5 C3 H5A H5C 0.3363 1.0406 0.8522 137 0.980 0.000 C5 C3 H5A H6A 0.0812 0.8678 0.9653 137 0.980 0.000 C6 N1 H6A H6B 0.0522 0.8322 0.8758 137 0.980 0.000 C6 N1 H6A H6C 0.0864 0.9513 0.8949 137 0.980 0.000 C6 N1 H6A H7A 0.5618 0.8722 1.0375 23 0.990 0.000 C7 C8 C2 H7B 0.6578 0.8968 0.9630 23 0.990 0.000 C7 C8 C2 H9 0.6595 1.0656 0.9093 43 0.950 0.000 C9 C8 C10 H10 0.5726 1.2340 0.8994 43 0.950 0.000 C10 C11 C9 H11 0.3678 1.2779 0.9623 43 0.950 0.000 C11 C10 C12 H12 0.2555 1.1543 1.0403 43 0.950 0.000 C12 C11 C13 H13 0.3441 0.9866 1.0527 43 0.950 0.000 C13 C12 C8 H14 0.5428 0.8714 0.7418 43 0.950 0.000 C14 N2 C15 H15 0.7200 0.7744 0.8560 43 0.950 0.000 C15 C16 C14 H16 0.7417 0.8154 0.6925 43 0.950 0.000 C16 C15 C17 H18 0.9003 0.6662 0.8494 43 0.950 0.000 C18 C19 C17 H19 1.0809 0.5494 0.8317 43 0.950 0.000 C19 C18 C20 H20 1.1788 0.5278 0.7057 43 0.950 0.000 C20 C21 C19 H21 1.0974 0.6235 0.5976 43 0.950 0.000 C21 C22 C20 H22 0.9188 0.7417 0.6147 43 0.950 0.000 C22 C21 C17 2008src0076 in P2(1)2(1)2(1) ATOM x y z sof U11 U22 U33 U23 U13 U12 Ueq C1 0.32979 0.81886 0.95671 1.00000 0.02778 0.01913 0.02220 -0.00125 0.00043 -0.00190 0.02304 0.00385 0.00025 0.00017 0.00012 0.00000 0.00126 0.00101 0.00106 0.00088 0.00096 0.00098 0.00049 C2 0.47791 0.82090 0.93061 1.00000 0.02923 0.02184 0.01628 0.00278 0.00234 0.00538 0.02245 0.00400 0.00025 0.00017 0.00012 0.00000 0.00125 0.00102 0.00091 0.00084 0.00093 0.00096 0.00047 H2 0.51808 0.74952 0.93394 1.00000 0.02694 0.00000 0.00000 C3 0.32224 0.88416 0.82470 1.00000 0.01874 0.02192 0.02254 0.00066 0.00076 0.00200 0.02106 0.00390 0.00025 0.00017 0.00012 0.00000 0.00112 0.00107 0.00100 0.00087 0.00086 0.00093 0.00046 C4 0.27163 0.81714 0.75586 1.00000 0.02631 0.03085 0.02742 -0.00592 -0.00165 -0.00021 0.02819 0.00405 0.00026 0.00019 0.00014 0.00000 0.00127 0.00118 0.00114 0.00101 0.00099 0.00105 0.00053 H4A 0.29601 0.74434 0.76563 1.00000 0.04229 0.00000 0.00000 H4B 0.31436 0.84062 0.70631 1.00000 0.04229 0.00000 0.00000 H4C 0.17201 0.82344 0.75142 1.00000 0.04229 0.00000 0.00000 C5 0.31338 0.99962 0.80493 1.00000 0.02552 0.02295 0.02603 0.00260 -0.00213 0.00366 0.02483 0.00410 0.00025 0.00017 0.00014 0.00000 0.00120 0.00104 0.00103 0.00094 0.00099 0.00102 0.00048 H5A 0.22022 1.01652 0.78772 1.00000 0.03725 0.00000 0.00000 H5B 0.37790 1.01601 0.76214 1.00000 0.03725 0.00000 0.00000 H5C 0.33633 1.04057 0.85221 1.00000 0.03725 0.00000 0.00000 C6 0.10586 0.87906 0.90953 1.00000 0.02079 0.03838 0.03793 0.00149 0.00503 0.00050 0.03237 0.00470 0.00026 0.00021 0.00015 0.00000 0.00127 0.00139 0.00133 0.00116 0.00107 0.00112 0.00058 H6A 0.08123 0.86785 0.96534 1.00000 0.04855 0.00000 0.00000 H6B 0.05223 0.83221 0.87577 1.00000 0.04855 0.00000 0.00000 H6C 0.08644 0.95132 0.89486 1.00000 0.04855 0.00000 0.00000 C7 0.56192 0.89723 0.98186 1.00000 0.02187 0.03500 0.02373 -0.00228 -0.00157 0.00553 0.02687 0.00401 0.00025 0.00018 0.00013 0.00000 0.00119 0.00120 0.00103 0.00099 0.00096 0.00101 0.00050 H7A 0.56175 0.87223 1.03752 1.00000 0.03224 0.00000 0.00000 H7B 0.65784 0.89676 0.96299 1.00000 0.03224 0.00000 0.00000 C8 0.50959 1.00771 0.98034 1.00000 0.02488 0.02842 0.02013 -0.00234 -0.00355 -0.00257 0.02448 0.00377 0.00024 0.00018 0.00013 0.00000 0.00121 0.00109 0.00097 0.00093 0.00093 0.00097 0.00049 C9 0.57689 1.08295 0.93589 1.00000 0.02736 0.04254 0.03057 -0.00093 0.00081 -0.01301 0.03349 0.00428 0.00028 0.00021 0.00015 0.00000 0.00139 0.00145 0.00121 0.00114 0.00108 0.00117 0.00059 H9 0.65955 1.06563 0.90931 1.00000 0.04019 0.00000 0.00000 C10 0.52491 1.18336 0.92978 1.00000 0.05403 0.03317 0.03224 0.00400 -0.00816 -0.02332 0.03981 0.00434 0.00033 0.00020 0.00016 0.00000 0.00185 0.00133 0.00125 0.00111 0.00133 0.00137 0.00068 H10 0.57256 1.23400 0.89938 1.00000 0.04777 0.00000 0.00000 C11 0.40443 1.20987 0.96764 1.00000 0.06214 0.02320 0.02973 -0.00357 -0.01303 -0.00290 0.03836 0.00444 0.00034 0.00020 0.00014 0.00000 0.00197 0.00117 0.00128 0.00106 0.00134 0.00128 0.00068 H11 0.36778 1.27794 0.96228 1.00000 0.04603 0.00000 0.00000 C12 0.33768 1.13630 1.01342 1.00000 0.04194 0.03002 0.02954 -0.00625 -0.00052 0.00470 0.03383 0.00448 0.00030 0.00019 0.00014 0.00000 0.00156 0.00126 0.00117 0.00109 0.00116 0.00117 0.00059 H12 0.25554 1.15432 1.04029 1.00000 0.04060 0.00000 0.00000 C13 0.39002 1.03618 1.02038 1.00000 0.03066 0.02466 0.02427 0.00017 0.00338 -0.00094 0.02653 0.00417 0.00026 0.00018 0.00014 0.00000 0.00128 0.00111 0.00107 0.00100 0.00103 0.00102 0.00050 H13 0.34408 0.98663 1.05266 1.00000 0.03183 0.00000 0.00000 C14 0.56108 0.84369 0.79304 1.00000 0.02622 0.01946 0.01920 0.00071 0.00086 0.00039 0.02163 0.00375 0.00024 0.00016 0.00012 0.00000 0.00121 0.00099 0.00096 0.00084 0.00092 0.00092 0.00046 H14 0.54277 0.87140 0.74180 1.00000 0.02595 0.00000 0.00000 C15 0.69006 0.79516 0.80470 1.00000 0.02163 0.02381 0.02130 0.00040 -0.00076 0.00234 0.02225 0.00380 0.00023 0.00017 0.00013 0.00000 0.00117 0.00106 0.00097 0.00090 0.00092 0.00095 0.00046 H15 0.71996 0.77442 0.85603 1.00000 0.02670 0.00000 0.00000 C16 0.76849 0.77978 0.73943 1.00000 0.02091 0.02170 0.02416 0.00049 -0.00235 -0.00114 0.02226 0.00381 0.00024 0.00017 0.00013 0.00000 0.00115 0.00101 0.00107 0.00090 0.00091 0.00092 0.00047 H16 0.74173 0.81543 0.69248 1.00000 0.02671 0.00000 0.00000 C17 0.88926 0.71445 0.73371 1.00000 0.01859 0.02063 0.02476 -0.00096 0.00148 -0.00269 0.02133 0.00375 0.00023 0.00017 0.00013 0.00000 0.00109 0.00100 0.00106 0.00091 0.00091 0.00093 0.00046 C18 0.93977 0.65744 0.79826 1.00000 0.02256 0.02763 0.02246 -0.00004 0.00090 0.00029 0.02422 0.00394 0.00024 0.00017 0.00013 0.00000 0.00118 0.00113 0.00102 0.00093 0.00095 0.00097 0.00048 H18 0.90033 0.66621 0.84943 1.00000 0.02906 0.00000 0.00000 C19 1.04723 0.58812 0.78783 1.00000 0.02519 0.02900 0.02702 0.00240 -0.00280 0.00388 0.02707 0.00412 0.00025 0.00018 0.00014 0.00000 0.00125 0.00115 0.00112 0.00098 0.00100 0.00104 0.00051 H19 1.08090 0.54936 0.83174 1.00000 0.03248 0.00000 0.00000 C20 1.10562 0.57548 0.71285 1.00000 0.02161 0.02618 0.03848 -0.00280 0.00286 0.00311 0.02876 0.00423 0.00026 0.00018 0.00014 0.00000 0.00119 0.00114 0.00133 0.00105 0.00106 0.00102 0.00053 H20 1.17878 0.52776 0.70569 1.00000 0.03451 0.00000 0.00000 C21 1.05724 0.63237 0.64862 1.00000 0.02510 0.03072 0.02885 -0.00277 0.00526 -0.00037 0.02822 0.00426 0.00026 0.00019 0.00014 0.00000 0.00128 0.00121 0.00113 0.00100 0.00100 0.00108 0.00053 H21 1.09736 0.62348 0.59765 1.00000 0.03387 0.00000 0.00000 C22 0.95059 0.70209 0.65868 1.00000 0.02375 0.02900 0.02266 0.00092 0.00154 -0.00083 0.02514 0.00399 0.00025 0.00018 0.00013 0.00000 0.00124 0.00115 0.00102 0.00094 0.00097 0.00104 0.00049 H22 0.91876 0.74168 0.61474 1.00000 0.03017 0.00000 0.00000 N1 0.25184 0.85786 0.89850 1.00000 0.02142 0.02201 0.02465 0.00075 0.00340 0.00145 0.02269 0.00331 0.00020 0.00014 0.00011 0.00000 0.00103 0.00094 0.00090 0.00079 0.00079 0.00080 0.00042 N2 0.46597 0.85340 0.84653 1.00000 0.02131 0.01927 0.01948 0.00040 0.00105 0.00441 0.02002 0.00323 0.00020 0.00014 0.00010 0.00000 0.00099 0.00084 0.00082 0.00072 0.00074 0.00082 0.00039 O1 0.29102 0.79039 1.02258 1.00000 0.03729 0.02811 0.02323 0.00332 0.00648 -0.00452 0.02955 0.00288 0.00018 0.00012 0.00009 0.00000 0.00100 0.00081 0.00079 0.00069 0.00075 0.00077 0.00039 B1_a 0.58135 1.01491 0.60528 0.66896 0.03841 0.03055 0.03397 0.01125 -0.01012 -0.00601 0.03431 0.01029 0.00065 0.00046 0.00035 0.00374 0.00228 0.00148 0.00170 0.00136 0.00167 0.00154 0.00089 F1_a 0.47235 0.94659 0.61792 0.66896 0.05127 0.05017 0.04968 -0.00111 0.00420 -0.01533 0.05038 0.01119 0.00071 0.00052 0.00058 0.00374 0.00219 0.00191 0.00113 0.00194 0.00156 0.00188 0.00105 F2_a 0.60425 1.02821 0.52601 0.66896 0.03782 0.12247 0.04413 0.03422 -0.00316 -0.00412 0.06814 0.01533 0.00074 0.00086 0.00029 0.00374 0.00249 0.00474 0.00203 0.00262 0.00184 0.00268 0.00178 F3_a 0.69459 0.96959 0.64100 0.66896 0.05789 0.04872 0.09483 0.03460 -0.04146 -0.00725 0.06715 0.01078 0.00063 0.00048 0.00049 0.00374 0.00338 0.00305 0.00427 0.00312 0.00316 0.00227 0.00169 F4_a 0.55659 1.10654 0.64287 0.66896 0.12787 0.02848 0.11119 -0.00833 -0.00120 0.00241 0.08918 0.01349 0.00090 0.00031 0.00045 0.00374 0.00504 0.00174 0.00409 0.00222 0.00339 0.00253 0.00162 B11_b 0.59761 1.01191 0.61535 0.15645 0.03841 0.03055 0.03397 0.01125 -0.01012 -0.00601 0.03431 0.02643 0.00181 0.00115 0.00091 0.00721 0.00228 0.00148 0.00170 0.00136 0.00167 0.00154 0.00089 F11_b 0.49088 0.94204 0.61550 0.15645 0.05127 0.05017 0.04968 -0.00111 0.00420 -0.01533 0.05038 0.03171 0.00253 0.00186 0.00160 0.00721 0.00219 0.00191 0.00113 0.00194 0.00156 0.00188 0.00105 F12_b 0.58969 1.07861 0.55299 0.15645 0.09422 0.05405 0.07272 0.04523 0.00815 0.00649 0.07366 0.03843 0.00229 0.00133 0.00118 0.00721 0.01011 0.00815 0.00929 0.00713 0.00878 0.00777 0.00488 F13_b 0.71811 0.95850 0.60353 0.15645 0.03973 0.04346 0.05791 0.00127 0.01240 0.00546 0.04703 0.03889 0.00195 0.00147 0.00106 0.00721 0.00626 0.00659 0.00907 0.00723 0.00720 0.00514 0.00403 F14_b 0.60101 1.06521 0.68553 0.15645 0.04819 0.05680 0.07998 -0.04237 0.00990 -0.01589 0.06165 0.02166 0.00170 0.00164 0.00106 0.00721 0.00850 0.01005 0.00872 0.00765 0.00721 0.00737 0.00500 B21_c 0.56254 1.01415 0.60977 0.17458 0.03841 0.03055 0.03397 0.01125 -0.01012 -0.00601 0.03431 0.02845 0.00172 0.00125 0.00101 0.00740 0.00228 0.00148 0.00170 0.00136 0.00167 0.00154 0.00089 F21_c 0.48976 0.92183 0.61518 0.17458 0.05127 0.05017 0.04968 -0.00111 0.00420 -0.01533 0.05038 0.03361 0.00241 0.00122 0.00194 0.00740 0.00219 0.00191 0.00113 0.00194 0.00156 0.00188 0.00105 F22_c 0.62734 1.01892 0.53811 0.17458 0.04822 0.12252 0.06613 0.02515 0.02940 -0.01794 0.07895 0.05351 0.00247 0.00260 0.00107 0.00740 0.01104 0.01300 0.00951 0.01069 0.00851 0.00939 0.00640 F23_c 0.65716 1.01634 0.67040 0.17458 0.07367 0.05593 0.09281 0.01837 -0.04199 -0.00429 0.07414 0.02787 0.00197 0.00155 0.00116 0.00740 0.01013 0.01023 0.00985 0.00833 0.00812 0.00801 0.00497 F24_c 0.47022 1.09316 0.61871 0.17458 0.11355 0.02979 0.05222 0.02104 0.01408 0.04274 0.06519 0.03762 0.00203 0.00101 0.00085 0.00740 0.01088 0.00578 0.00694 0.00508 0.00729 0.00710 0.00455 Final Structure Factor Calculation for 2008src0076 in P2(1)2(1)2(1) Total number of l.s. parameters = 344 Maximum vector length = 511 Memory required = 4334 / 27090 wR2 = 0.1029 before cycle 36 for 2740 data and 2 / 344 parameters Summary of restraints applied in cycle 36 ANTIBUMP DFIX DANG SAME/SADI CHIV/Z CHIV/NZ FLAT DELU SIMU ISOR SUMP Number 0. 12. 16. 30. 0. 0. 0. 30. 330. 0. 1. rms sigma 0.000 0.015 0.015 0.033 0.000 0.000 0.000 0.020 0.039 0.000 0.000 rms deviation 0.000 0.012 0.016 0.028 0.000 0.000 0.000 0.011 0.030 0.000 0.000 GooF = S = 1.049; Restrained GooF = 1.010 for 419 restraints Weight = 1 / [ sigma^2(Fo^2) + ( 0.0511 * P )^2 + 0.53 * P ] where P = ( Max ( Fo^2, 0 ) + 2 * Fc^2 ) / 3 R1 = 0.0418 for 2295 Fo > 4sig(Fo) and 0.0557 for all 2740 data wR2 = 0.1029, GooF = S = 1.049, Restrained GooF = 1.010 for all data Absolute structure cannot be determined reliably Occupancy sum of asymmetric unit = 30.00 for non-hydrogen and 25.00 for hydrogen atoms Principal mean square atomic displacements U 0.0283 0.0225 0.0184 C1 0.0327 0.0195 0.0151 C2 0.0237 0.0218 0.0177 C3 0.0354 0.0268 0.0224 C4 0.0282 0.0275 0.0188 C5 0.0405 0.0372 0.0194 C6 0.0375 0.0233 0.0197 C7 0.0298 0.0264 0.0173 C8 0.0501 0.0305 0.0199 C9 0.0712 0.0302 0.0180 C10 0.0668 0.0286 0.0197 C11 0.0441 0.0344 0.0231 C12 0.0322 0.0247 0.0227 C13 0.0264 0.0199 0.0186 C14 0.0253 0.0218 0.0197 C15 0.0256 0.0217 0.0194 C16 0.0257 0.0217 0.0167 C17 0.0276 0.0234 0.0216 C18 0.0315 0.0290 0.0207 C19 0.0394 0.0276 0.0193 C20 0.0343 0.0291 0.0212 C21 0.0292 0.0248 0.0214 C22 0.0272 0.0219 0.0190 N1 0.0250 0.0193 0.0157 N2 0.0406 0.0297 0.0183 O1 0.0530 0.0294 0.0205 B1_a 0.0669 0.0492 0.0351 F1_a 0.1356 0.0379 0.0309 F2_a 0.1346 0.0456 0.0212 F3_a 0.1281 0.1119 0.0276 F4_a 0.0530 0.0294 0.0205 B11_b 0.0669 0.0492 0.0351 F11_b 0.1148 0.0890 0.0172 F12_b 0.0648 0.0445 0.0318 F13_b 0.1168 0.0457 0.0225 F14_b 0.0530 0.0294 0.0205 B21_c 0.0669 0.0492 0.0351 F21_c 0.1327 0.0861 0.0181 F22_c 0.1303 0.0560 0.0362 F23_c 0.1369 0.0515 0.0071 F24_c Analysis of variance for reflections employed in refinement K = Mean[Fo^2] / Mean[Fc^2] for group Fc/Fc(max) 0.000 0.024 0.038 0.050 0.063 0.078 0.096 0.118 0.154 0.217 1.000 Number in group 280. 274. 268. 280. 270. 286. 260. 277. 269. 276. GooF 0.952 1.092 1.087 1.049 1.157 1.024 1.022 0.962 0.994 1.137 K 0.992 0.947 0.954 0.952 1.001 1.000 1.013 1.009 1.013 0.985 Resolution(A) 0.77 0.80 0.83 0.87 0.92 0.98 1.06 1.17 1.34 1.71 inf Number in group 274. 279. 270. 276. 276. 273. 272. 270. 275. 275. GooF 1.025 0.913 1.005 0.994 0.992 1.030 0.974 0.919 1.186 1.371 K 0.996 0.987 1.014 1.004 0.997 1.004 1.015 1.015 1.034 0.970 R1 0.145 0.131 0.110 0.096 0.067 0.044 0.036 0.031 0.033 0.031 Recommended weighting scheme: WGHT 0.0508 0.5271 Note that in most cases convergence will be faster if fixed weights (e.g. the default WGHT 0.1) are retained until the refinement is virtually complete, and only then should the above recommended values be used. Most Disagreeable Reflections (* if suppressed or used for Rfree) h k l Fo^2 Fc^2 Delta(F^2)/esd Fc/Fc(max) Resolution(A) 0 2 1 448.74 586.34 4.13 0.218 6.01 9 3 0 17.46 54.47 3.67 0.066 1.05 0 4 7 2.95 11.98 3.48 0.031 1.92 3 7 5 19.08 8.06 3.28 0.026 1.45 3 11 3 195.30 252.08 3.25 0.143 1.08 8 5 0 33.20 61.16 3.23 0.070 1.10 4 4 1 85.94 60.84 3.20 0.070 1.93 3 1 11 185.72 145.53 3.16 0.109 1.38 4 5 15 5.06 15.67 3.16 0.036 0.95 5 12 6 60.62 93.46 3.12 0.087 0.89 7 1 1 90.23 63.59 3.12 0.072 1.38 5 2 1 305.40 246.74 3.05 0.141 1.86 3 3 14 0.20 6.31 3.03 0.023 1.09 3 6 6 68.50 94.19 3.00 0.087 1.51 5 1 1 811.42 681.08 2.99 0.235 1.92 0 6 1 29.35 17.03 2.97 0.037 2.13 0 6 2 73.41 51.50 2.93 0.065 2.08 1 4 7 143.75 112.97 2.90 0.096 1.89 2 12 4 94.79 125.45 2.90 0.101 1.02 2 12 10 225.84 165.40 2.88 0.116 0.89 3 12 11 47.80 77.15 2.82 0.079 0.85 1 2 0 8639.13 10262.39 2.81 0.911 5.37 0 2 7 672.26 797.79 2.80 0.254 2.25 0 0 4 2368.87 2771.67 2.79 0.474 4.21 5 1 4 827.34 704.94 2.78 0.239 1.76 4 1 6 378.54 456.06 2.78 0.192 1.82 0 2 3 901.34 1061.45 2.77 0.293 4.23 0 4 9 1020.82 867.20 2.76 0.265 1.62 2 0 8 175.38 137.99 2.75 0.106 1.93 2 2 9 265.69 219.18 2.74 0.133 1.68 7 1 15 49.89 30.57 2.68 0.050 0.87 1 5 8 387.19 326.22 2.66 0.162 1.61 1 0 5 467.26 552.57 2.66 0.211 3.18 3 4 3 180.43 221.24 2.66 0.134 2.12 5 14 4 18.40 38.13 2.64 0.056 0.82 0 1 3 860.63 1008.77 2.62 0.286 5.14 12 1 7 -5.61 22.34 2.62 0.043 0.77 5 11 9 120.62 88.42 2.61 0.085 0.88 6 11 11 12.17 30.26 2.60 0.049 0.81 10 3 3 102.18 136.71 2.58 0.105 0.94 4 6 0 640.68 543.88 2.56 0.210 1.61 5 5 3 798.77 687.49 2.56 0.236 1.50 5 4 19 69.35 44.08 2.55 0.060 0.78 8 7 0 129.32 167.50 2.54 0.116 1.02 2 3 18 2.95 15.53 2.54 0.035 0.90 2 6 2 212.32 176.34 2.52 0.119 1.91 9 8 7 16.09 37.49 2.51 0.055 0.84 5 3 16 8.19 18.96 2.51 0.039 0.91 4 5 14 55.94 75.47 2.49 0.078 0.99 7 9 1 6.40 18.27 2.49 0.038 1.00 Bond lengths and angles C1 - Distance Angles O1 1.2270 (0.0026) N1 1.3384 (0.0029) 126.64 (0.23) C2 1.5132 (0.0034) 124.25 (0.21) 109.02 (0.18) C1 - O1 N1 C2 - Distance Angles N2 1.4797 (0.0026) C1 1.5132 (0.0034) 101.94 (0.18) C7 1.5431 (0.0033) 113.36 (0.19) 110.98 (0.18) H2 1.0000 110.10 110.10 110.10 C2 - N2 C1 C7 C3 - Distance Angles N1 1.4594 (0.0028) N2 1.5051 (0.0030) 99.88 (0.16) C5 1.5241 (0.0031) 112.62 (0.19) 111.24 (0.19) C4 1.5261 (0.0031) 111.22 (0.19) 109.84 (0.19) 111.47 (0.19) C3 - N1 N2 C5 C4 - Distance Angles C3 1.5261 (0.0031) H4A 0.9800 109.47 H4B 0.9800 109.47 109.47 H4C 0.9800 109.47 109.47 109.47 C4 - C3 H4A H4B C5 - Distance Angles C3 1.5241 (0.0031) H5A 0.9800 109.47 H5B 0.9800 109.47 109.47 H5C 0.9800 109.47 109.47 109.47 C5 - C3 H5A H5B C6 - Distance Angles N1 1.4646 (0.0031) H6A 0.9800 109.47 H6B 0.9800 109.47 109.47 H6C 0.9800 109.47 109.47 109.47 C6 - N1 H6A H6B C7 - Distance Angles C8 1.5103 (0.0032) C2 1.5431 (0.0033) 114.12 (0.19) H7A 0.9900 108.73 108.73 H7B 0.9900 108.73 108.73 107.63 C7 - C8 C2 H7A C8 - Distance Angles C9 1.3885 (0.0034) C13 1.3978 (0.0034) 118.25 (0.22) C7 1.5103 (0.0032) 120.28 (0.22) 121.42 (0.21) C8 - C9 C13 C9 - Distance Angles C8 1.3885 (0.0034) C10 1.3915 (0.0039) 120.89 (0.25) H9 0.9500 119.55 119.55 C9 - C8 C10 C10 - Distance Angles C11 1.3817 (0.0044) C9 1.3915 (0.0039) 120.41 (0.24) H10 0.9500 119.80 119.80 C10 - C11 C9 C11 - Distance Angles C10 1.3817 (0.0044) C12 1.3835 (0.0038) 119.34 (0.25) H11 0.9500 120.33 120.33 C11 - C10 C12 C12 - Distance Angles C11 1.3835 (0.0038) C13 1.3905 (0.0034) 120.43 (0.26) H12 0.9500 119.78 119.78 C12 - C11 C13 C13 - Distance Angles C12 1.3905 (0.0034) C8 1.3978 (0.0034) 120.64 (0.23) H13 0.9500 119.68 119.68 C13 - C12 C8 C14 - Distance Angles N2 1.3000 (0.0029) C15 1.4203 (0.0032) 125.56 (0.20) H14 0.9500 117.22 117.22 C14 - N2 C15 C15 - Distance Angles C16 1.3538 (0.0031) C14 1.4203 (0.0032) 117.06 (0.20) H15 0.9500 121.47 121.47 C15 - C16 C14 C16 - Distance Angles C15 1.3538 (0.0031) C17 1.4521 (0.0032) 126.78 (0.20) H16 0.9500 116.61 116.61 C16 - C15 C17 C17 - Distance Angles C18 1.4002 (0.0031) C22 1.4065 (0.0030) 119.12 (0.21) C16 1.4521 (0.0032) 122.56 (0.20) 118.12 (0.20) C17 - C18 C22 C18 - Distance Angles C19 1.3888 (0.0032) C17 1.4002 (0.0031) 120.32 (0.21) H18 0.9500 119.84 119.84 C18 - C19 C17 C19 - Distance Angles C18 1.3888 (0.0032) C20 1.3942 (0.0033) 119.92 (0.21) H19 0.9500 120.04 120.04 C19 - C18 C20 C20 - Distance Angles C21 1.3880 (0.0035) C19 1.3942 (0.0033) 120.23 (0.22) H20 0.9500 119.89 119.89 C20 - C21 C19 C21 - Distance Angles C22 1.3854 (0.0034) C20 1.3880 (0.0035) 120.16 (0.22) H21 0.9500 119.92 119.92 C21 - C22 C20 C22 - Distance Angles C21 1.3854 (0.0034) C17 1.4065 (0.0029) 120.23 (0.21) H22 0.9500 119.89 119.89 C22 - C21 C17 N1 - Distance Angles C1 1.3384 (0.0029) C3 1.4594 (0.0028) 116.17 (0.19) C6 1.4646 (0.0031) 122.13 (0.20) 121.61 (0.20) N1 - C1 C3 N2 - Distance Angles C14 1.3000 (0.0029) C2 1.4797 (0.0026) 125.33 (0.20) C3 1.5051 (0.0030) 121.60 (0.18) 112.41 (0.17) N2 - C14 C2 O1 - Distance Angles C1 1.2270 (0.0026) O1 - B1_a - Distance Angles F4_a 1.3590 (0.0059) F2_a 1.3632 (0.0054) 112.07 (0.50) F3_a 1.3878 (0.0055) 107.74 (0.49) 110.20 (0.51) F1_a 1.3972 (0.0053) 109.79 (0.49) 110.67 (0.47) 106.16 (0.45) B1_a - F4_a F2_a F3_a F1_a - Distance Angles B1_a 1.3972 (0.0054) F1_a - F2_a - Distance Angles B1_a 1.3632 (0.0054) F2_a - F3_a - Distance Angles B1_a 1.3878 (0.0055) F3_a - F4_a - Distance Angles B1_a 1.3590 (0.0059) F4_a - B11_b - Distance Angles F12_b 1.3574 (0.0106) F14_b 1.3657 (0.0104) 110.65 (1.09) F11_b 1.3769 (0.0103) 111.75 (1.18) 110.13 (1.12) F13_b 1.3779 (0.0107) 104.61 (1.36) 110.74 (1.06) 108.83 (1.12) B11_b - F12_b F14_b F11_b F11_b - Distance Angles B11_b 1.3769 (0.0104) F11_b - F12_b - Distance Angles B11_b 1.3574 (0.0105) F12_b - F13_b - Distance Angles B11_b 1.3779 (0.0107) F13_b - F14_b - Distance Angles B11_b 1.3657 (0.0104) F14_b - B21_c - Distance Angles F22_c 1.3634 (0.0102) F24_c 1.3673 (0.0104) 111.74 (1.09) F23_c 1.3772 (0.0104) 110.00 (1.08) 110.28 (1.03) F21_c 1.3871 (0.0103) 109.57 (1.09) 106.88 (1.03) 108.26 (1.06) B21_c - F22_c F24_c F23_c F21_c - Distance Angles B21_c 1.3871 (0.0104) F21_c - F22_c - Distance Angles B21_c 1.3634 (0.0102) F22_c - F23_c - Distance Angles B21_c 1.3772 (0.0104) F23_c - F24_c - Distance Angles B21_c 1.3673 (0.0104) F24_c - FMAP and GRID set by program FMAP 2 3 21 GRID -1.389 -2 -2 1.389 2 2 R1 = 0.0557 for 2740 unique reflections after merging for Fourier Electron density synthesis with coefficients Fo-Fc Highest peak 0.18 at 0.5463 0.5792 0.1624 [ 1.11 A from H6C ] Deepest hole -0.20 at 0.0156 0.1157 0.1341 [ 0.58 A from F21 ] Mean = 0.00, Rms deviation from mean = 0.04 e/A^3, Highest memory used = 4149 / 22524 Fourier peaks appended to .res file x y z sof U Peak Distances to nearest atoms (including symmetry equivalents) Q1 1 0.0463 0.9208 0.8376 1.00000 0.05 0.18 1.11 H6C 1.31 H6B 1.45 C6 2.26 H5A Q2 1 0.4416 1.0143 0.5949 1.00000 0.05 0.16 1.00 F1 1.10 F11 1.13 F24 1.21 B21 Q3 1 0.0694 0.8064 0.9351 1.00000 0.05 0.15 0.95 H6A 1.07 H6B 1.09 C6 1.99 H6C Q4 1 0.5637 0.9206 0.6102 1.00000 0.05 0.15 0.73 F21 0.77 F11 0.96 F1 1.20 B21 Q5 1 0.1158 0.9445 0.9500 1.00000 0.05 0.15 0.97 H6C 1.07 H6A 1.09 C6 1.94 N1 Shortest distances between peaks (including symmetry equivalents) 2 4 1.72 3 5 1.85 1 5 2.03 1 3 2.21 2 5 2.56 Time profile in seconds ----------------------- 0.07: Read and process instructions 0.00: Fit rigid groups 0.01: Interpret restraints etc. 0.00: Generate connectivity array 0.01: Analyse DFIX/DANG restraints 0.00: Analyse SAME/SADI restraints 0.00: Generate CHIV restraints 0.00: Check if bonds in residues restrained 0.00: Generate DELU restraints 0.00: Generate SIMU restraints 0.00: Generate ISOR restraints 0.00: Generate NCSY restraints 0.01: Analyse other restraints etc. 2.13: Read intensity data, sort/merge etc. 0.00: Set up constraints 0.01: OSF, H-atoms from difference map 0.03: Set up l.s. refinement 0.01: Generate idealized H-atoms 12.91: Structure factors and derivatives 18.08: Sum l.s. matrices 0.00: Generate and apply antibumping restraints 0.63: Apply other restraints 4.30: Solve l.s. equations 0.00: Generate HTAB table 0.18: Other dependent quantities, CIF, tables 0.04: Analysis of variance 0.03: Merge reflections for Fourier and .fcf 0.03: Fourier summations 0.05: Peaksearch 0.00: Analyse peaklist +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + 2008src0076 finished at 10:22:24 Total CPU time: 38.4 secs + +++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++